Process for carrying out a hydrogenation reaction and removing pyrophoric catalyst

ABSTRACT

A batch process for carrying out a hydrogenation reaction comprises mixing a pyrophoric catalyst with reactants and solvents to form a reaction mixture in a reaction vessel. Hydrogen is added to the reaction vessel. After hydrogenation, the desired hydrogenation product is removed from the reaction vessel and the pyrophoric catalyst-rich material from the reaction vessel is delivered to a pressure filter. Water is added to the pyrophoric catalyst-rich material in the filter and the spent pyrophoric material is removed from the pressure filter in a water wet form.

RELATED APPLICATIONS

This application is a continuation application of U.S. Ser. No.10/172,058, filed Jun. 14, 2002, now pending, which is a continuation ofPCT/IE00/00156, filed Dec. 18, 2000, which claims benefit ofPCT/IE99/00137, filed Dec. 17, 1999, all of which are incorporatedherein by reference in their entirety.

FIELD OF THE INVENTION

The invention relates to a factory scale apparatus for carrying out ahydrogenation reaction.

BACKGROUND OF THE INVENTION

Hydrogenation reactions are frequently carried out in the presence of apyrophoric catalyst such as Raney nickel. This presents a seriousdifficulty because flammable liquids such as methanol or ethanol areoften used as hydrogenation solvents. The removal of the catalyst fromthe reaction mixture after the hydrogenation reaction is complete,presents serious difficulties. Generally the reaction mixture is passedthrough a filter, the catalyst is filtered out and removed in a closedcircuit.

Handling of the resultant catalyst presents difficulties and thecommonly used multiplate filters, which necessitate generation ofhazardous dry material, require extensive safety precautions, andextended operation times to facilitate safe removal of the catalyst.

U.S. Pat. No. 4,021,354 describes a pressure filter comprising an outercasing having a filter basket supported therein. The filter basketcomprises a tubular imperforate metallic shell with a sintered stainlesssteel filter disc welded to the lower end of the shell. Such a pressurefilter is not suitable for use with fine metallic catalyst as thesintered disc readily clogs during operation. Removal of catalyst fromthe pores requires reverse flow of water and frequent use of acid todissolve trapped material.

DE-A-3136905 describes a pressure filter including a sieve basket of thesame type as that described in U.S. Pat. No. 4,021,354 and similardisadvantages apply.

There is therefore a need for an improved cost effective filterapparatus for removing a pyrophoric catalyst which will overcome theseproblems.

SUMMARY OF THE INVENTION

According to the invention there is provided a filter apparatus forrecovery of spent hydrogenation catalyst-rich material, the apparatuscomprising:

(a) a pressure filter container;

(b) the container having a filter plate mounted therein on whichpyrophoric catalyst-rich material is filtered;

(c) the container having a catalyst inlet for pyrophoric catalyst-richmaterial to be filtered and an inlet for delivery of solvent or water towash the spent catalyst on the filter plate; and

(d) a filter bag of solvent/water permeable material mounted in thecontainer and supported on the filter plate for collection of filteredspent pyrophoric catalyst material in a water-wet form.

In a preferred embodiment the filter bag is of flexible materialallowing easy fitting and removal from the filter. The bag can be foldedinto a compact size for disposal when required. Ideally the bag is ofmultifilament woven material. This ensures a large multilayer filtersurface area which is not prone to blockage.

In a particularly preferred embodiment of the invention the bag is ofacid resistant polypropylene multifilament weave. Thus if blockagesoccur the filter can be reversed and flushed with high pressure waterand if necessary soaked in dilute HCl acid. Alternatively, the bags maybe replaced at a predetermined frequency.

In one embodiment the filter bag is releasably mounted to the container.Preferably the filter apparatus includes releasable mounting means fortightening and demounting the filter bag from the container. The bag maybe fitted with sewn lifting straps and removed by hoist into drums foroff-site recovery of catalyst.

The filter container is preferably mounted on a transportable chassis.Preferably the chassis is a wheeled chassis.

The apparatus may be used in a batch process for carrying out ahydrogenation reaction comprising the steps of:

(a) mixing a pyrophoric catalyst with reactants and solvents to form areaction mixture in a reaction vessel;

(b) adding hydrogen to the reaction vessel;

(c) after hydrogenation, removing the desired hydrogenation product fromthe reaction vessel;

(d) delivering the pyrophoric catalyst-rich material from the reactionvessel to a pressure filter;

(e) adding water to the pyrophoric catalyst-rich material in the filter;and

(f) removing the spent pyrophoric material from the pressure filter in awater wet form.

In a preferred embodiment of the invention the pressure filter is asingle plate pressure filter, the catalyst being held in the filter in awater wet form.

In one embodiment the catalyst is Raney nickel.

Preferably the contents of the reaction vessel are decanted afterhydrogenation, the desired hydrogenation product being substantiallyremoved while allowing the catalyst-rich material to settle at thebottom of the vessel.

Preferably the reaction vessel is an agitated vessel, the agitator beingstopped to allow the catalyst to settle at the bottom of the vessel.

In one embodiment of the invention the process includes the step ofwashing the catalyst-rich material in the filter with a solvent torecover residual desired hydrogenation product.

The pressure filter may be fitted with a removable filter bag and inthis case the water wet catalyst is preferably removed from the bag andthe bag is reusable. Alternatively the bag containing the catalyst isremoved and sent for catalyst recovery.

DESCRIPTION OF THE DRAWINGS

The invention will be more clearly understood from the followingdescription given by way of example only with reference to theaccompanying drawings in which:

FIG. 1 is a perspective view from the front of a filter apparatus of theinvention;

FIG. 2 is a perspective view from the side of the filter apparatus ofFIG. 1;

FIG. 3A is an exploded perspective view of a removable filter bag andassociated clamping band;

FIG. 3B is a perspective view of the filter bag in position;

FIG. 4 is a top view of a clam-shell lid of the filter apparatus of FIG.1; and

FIG. 5 is a cross-sectional view of the filter apparatus of theinvention.

DETAILED DESCRIPTION OF THE INVENTION

The invention will be more clearly understood from the followingdescription given by way of example only.

The invention utilizes a process wherein, after hydrogenation, areaction mixture is decanted, the desired hydrogenation product issubstantially removed and catalyst-rich material which settles at thebottom of the vessel is delivered to a single plate pressure filter. Thespent catalyst is retained in the filter bag while the product richsolvent is led away from the bottom outlet of the pressure filter to areceiving vessel. The retained catalyst material is washed with asolvent to recover residual product and then washed with water tosaturate the catalyst material which is then safely and easilytransferred to drums and stored under water awaiting recovery.

Referring to FIGS. 1 to 5 there is illustrated a filter apparatus 1 ofthe invention. The filter apparatus 1 comprises a container having adomed base 2, a generally cylindrical sidewall 3 terminating in an upperrim 4 closed by a removable lid 5 having lifting lugs 6. The lid 5 isfixed in pressure-tight engagement with the sidewall 3 by flangeengaging screw clamps 7 and an embedded polytetrafluoroethene gasket 8.

The filter container has a single removable, perforated filter plate 9which is supported in spaced-apart relation from the base 2 by supports12. The base 2 has an outlet 10 below the filter plate 9. The outlet 10is fitted with an outlet valve 13 for discharge of product-rich solvent.

The lid 5 has several fittings including a main catalyst inlet line 15,a decant inlet valve 16, and a water wash inlet line 17. A light port18, a sight glass 19, pressure relief line 20, and a nitrogen purge line21 are also provided. An earth clip 22 is located on the lid 5.

The filter container has two jacketed coils 30 with inlet and outlets31, 32. The jackets may be heated or cooled, as required, to heat orcool the contents of the filter container. A hot water pressure releasedevice 23 and a hot water overflow 27 are also provided.

Referring especially to FIG. 3 there is illustrated a removable filterbag 40 of water/solvent permeable material, typically of acid resistantpolypropylene weave (about 10-micron pores), with a top rim 41 held inposition against the side wall 3 of the filter container by a band 11. Areleasable ring clamp 42 is provided on the band 11. The clamp 42 isadjustable to maximize the diameter of band 11 and thus tighten thefilter bag rim 41 against the filter side wall 3. The bottom of thefilter bag 40 rests on a perforated filter plate 9 which is supported bya filter plate support 12. The filter is inerted by first applying avacuum and then breaking the vacuum with nitrogen. Most of the contentsof a reaction vessel after settling are pressure decanted from thereaction vessel and fed into the closed single plate pressure filterapparatus 1 through an inlet line 16. Liquid free of catalyst isdischarged through the bottom outlet valve 13 and transferred to areceiving vessel. The residual catalyst in the reaction vessel is fed tothe filter through the larger inlet line 15 followed by a solvent washto recover residual product. The spent catalyst is retained in a filterbag 40 while the desired product is drained off and removed, by applyingpressure to the apparatus 1, through to a receiving vessel via theoutlet valve 13. Water is then added through the wash inlet line 17 towash out residual solvent to waste and to saturate the retained catalystmaterial. The pressure in the filter apparatus 1 is released and the lid5 is removed by passing a chain through the lugs 6 and hoisting the lid5 off. Water saturated catalyst is scooped directly to drums and storedunder water. Alternatively the filter bag 40 is lifted out and the waterwet catalyst is removed and stored for disposal. The filter bag 40 maybe reused. Alternatively the filter bag 40 is lifted out of the pressurefilter and the bag containing catalyst charged to a drum where it isstored under water and sent for catalyst recovery.

The filter container is mounted on a wheeled chassis 50 so that thefilter apparatus may be easily moved from one location to another.

The invention provides a simple, cheap and rapid method for removingspent pyrophoric catalyst from hydrogenation catalyst-rich material. Thefilter apparatus is cheap to set up and maintain. By keeping thepyrophoric catalyst water wet the catalyst does not pose a safety hazardand may be easily taken from the filter apparatus 1 in removable filterbags 40 and safely and easily transferred to drums containing water forstorage and recovery. The filter surface area is readily cleaned andreused or alternatively is disposable.

The invention is not limited to the embodiments hereinbefore describedwhich may be varied in detail.

What is claimed is:
 1. A batch process for carrying out a hydrogenationreaction comprising the steps of: (a) providing a reaction vessel; (b)mixing a pyrophoric catalyst with reactants and solvents to form areaction mixture in the reaction vessel; (c) adding hydrogen to thereaction vessel; (d) after hydrogenation, removing the desiredhydrogenation product from the reaction vessel and retaining pyrophoriccatalyst-rich material in the vessel; (e) providing a pressure filtercomprising a container having an upper rim closable by a removable lid,the lid having a main inlet for pyrophoric catalyst-rich material; (f)mounting a removable filter bag in the container; (g) closing the lid;(h) delivering the pyrophoric catalyst-rich material from the reactionvessel through the main inlet to the removable filter bag; (i) addingwater to the pyrophoric catalyst-rich material in the filter bag tosaturate the pyrophoric catalyst-rich material in the filter bag; (j)opening the lid of the pressure filter; and (k) removing the filter bagcontaining the spent pyrophoric catalyst-rich material from the pressurefilter in a water wet form.
 2. A process as claimed in claim 1comprising washing the catalyst-rich material in the filter bag with asolvent to recover residual desired hydrogenation product.
 3. A processas claimed in claim 1 wherein the pressure filter is a single platepressure filter, and the process comprises holding the catalyst in thefilter in a water wet form.
 4. A process as claimed in claim 1 whereinthe catalyst is Raney Nickel.
 5. A process as claimed in claim 1comprising decanting the contents of the reaction vessel afterhydrogenation, the desired hydrogenation product being substantiallyremoved while allowing the catalyst-rich material to settle in thebottom of the vessel.
 6. A process as claimed in claim 1 wherein thereaction vessel has an agitator and the process comprises the step ofstopping the agitator to allow the catalyst to settle at the bottom ofthe vessel.